摘要
为探索异(噁)唑草酮绿色合成工艺,采用甲苯作为单一溶剂进行回收套用,以2-硝基-4-三氟甲基苯腈为起始原料,经甲硫基化、氧化、加成缩合水解、烯醇化和环合共6步反应合成了异(噁)唑草酮,并优化了各步反应条件.优化条件下,甲硫基化收率96.6％、氧化收率97.9％、与环丙基甲基酮加成缩合水解收率95.0％、6步反应总收率78.5％,产品纯度98.0％.该工艺原料廉价易得,操作简单,中间体无需分离纯化,适合工业化生产.
Abstract
To explore the green synthesis process of isoxaflutole,toluene was used as a single solvent for recycling and reusing.Starting from 2-nitro-4-(trifluoromethyl)benzonitrile,isoxaflutole was synthesized through six steps of methylthiolation,oxidation,addition-condensation,hydrolyzation,enolization and cyclization.The reaction conditions for each step were optimized.Under the optimized conditions,the yields of methylthiolation,oxidation,and addition-condensation-hydrolyzation with cyclopropyl methyl ketone were 96.6％,97.9％and 95.0％.The total yield of the six-step reaction was 78.5％,and the product purity was 98.0％.This process uses inexpensive and readily available raw materials,has simple operation,circumvents separation and purification of intermediates,and is suitable for industrial production.
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